HRID26661

反应详情

EQUATION

反应方程式

HRID 26661 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 100 volume parts of dry tetrahydrofuran are added 4.28 parts of comminuted anhydrous aluminum chloride, 2.50 parts of 4-oxo-4H-1-benzopyran-3-carbonitrile and 4.18 parts of sodium azide in this order and, the whole mixture is refluxed under stirring for 23 hours. Then, to the resulting mixture 35 volume parts of 15 weight% hydrochloric acid are added, followed by distilling off tetrahydrofuran under reduced pressure. The resulting solid residue is recovered by filtration and recrystallized from dimethylformamide. This procedure yields 3-(1H-tetrazol-5-yl) chromone as colorless hairy needles. Melting point: 284°-285° C.(decomp. with foaming).

WORKUP

后处理

  1. temperaturethe whole mixture is refluxed
  2. distillationby distilling off tetrahydrofuran under reduced pressure
  3. filtrationThe resulting solid residue is recovered by filtration
  4. customrecrystallized from dimethylformamide